CN102701138A - Large-area layered etching and transferring method for metal-assisted silicon nanowire array - Google Patents
Large-area layered etching and transferring method for metal-assisted silicon nanowire array Download PDFInfo
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- CN102701138A CN102701138A CN2012101266535A CN201210126653A CN102701138A CN 102701138 A CN102701138 A CN 102701138A CN 2012101266535 A CN2012101266535 A CN 2012101266535A CN 201210126653 A CN201210126653 A CN 201210126653A CN 102701138 A CN102701138 A CN 102701138A
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 125
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 125
- 239000010703 silicon Substances 0.000 title claims abstract description 125
- 239000002070 nanowire Substances 0.000 title claims abstract description 77
- 238000005530 etching Methods 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 38
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 20
- 239000002184 metal Substances 0.000 title claims abstract description 20
- 239000002105 nanoparticle Substances 0.000 claims abstract description 13
- 239000003054 catalyst Substances 0.000 claims abstract description 10
- 239000000758 substrate Substances 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 238000001039 wet etching Methods 0.000 claims abstract description 3
- 238000012546 transfer Methods 0.000 claims description 13
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 8
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000003325 tomography Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000011943 nanocatalyst Substances 0.000 claims description 5
- 238000005498 polishing Methods 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000007747 plating Methods 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims 2
- 229910052709 silver Inorganic materials 0.000 claims 2
- 239000004332 silver Substances 0.000 claims 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 210000000498 stratum granulosum Anatomy 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 4
- 239000002390 adhesive tape Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000000126 substance Substances 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000007772 electroless plating Methods 0.000 description 3
- 229910014299 N-Si Inorganic materials 0.000 description 2
- 230000008033 biological extinction Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000000137 annealing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000003863 metallic catalyst Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
The invention discloses a large-area layered etching and transferring method of a metal-assisted silicon nanowire array, which is characterized in that a Si sheet subjected to primary wet etching is heated in air to partially melt an Ag nanoparticle catalyst at the bottom of the silicon nanowire array, partial Ag nanoparticles are adhered to the side wall of the silicon nanowire array, the adhered Ag nanoparticles are transversely etched in the secondary etching process, so that the silicon nanowire array generates a regular fault through secondary etching reaction, and then the silicon nanowire array on the fault is stripped by using an adhesive tape. The invention provides a method for layered etching and transferring of a silicon nanowire array for industrial production, which can realize the full utilization of a silicon substrate material of a body and the manufacture of a flexible silicon nanometer device.
Description
Technical field
The present invention relates to field of nano material preparation; Be specifically related to a kind of metal auxiliary silicon nano-wire array large tracts of land layering etching and transfer method; Utilize metal catalytic electroless plating chemical method etching silicon nano line array technique; Direct-fired method is handled metallic catalyst in the employing air, makes silicon nanowire array in secondarily etched reaction, produce a neat tomography through etching, and utilizes the method for this tomography transferred silicon nano-wire array.
Background technology
Silicon nanowires (silicon nanowires; SiNWs) typical case as the one dimension silicon nano material represents; Remove and have the special nature that conventional semiconductor material has; Also demonstrate physical property and the chemical property such as field emission, thermal conductivity, visible photoluminescent and catalysis that are different from the body silicon materials, have a huge application at aspects such as nano electron device, opto-electronic device and new forms of energy potential.Through utilizing the good light absorption of silicon nanowire array (fall in luminous effect), and the efficient carrier separation and the transport capability that bring of p-n junction radially, silicon nanowire array shows important application prospects in photovoltaic device of new generation.
People such as Peng Kui celebrating in 2006 have invented the method for metal catalytic electroless plating chemical method etch silicon nanometer, and the method is a direct growth on silicon base, does not need outside silicon source, and silicon nanowire array is formed by the direct etch silicon substrate of etching liquid.This method is applicable to that the large tracts of land of silicon nanowire array is synthetic, not only with low cost, method is simple, is easy to control, and repeatability better.
In application facet, because the excellent extinction ability of silicon nanowire array, very hundreds of microns monocrystal silicon substrate of the extinction ability of thin silicon nano-wire array (about 10 microns) and tradition are suitable, and the thickness of this meaning silicon nanowire array photovoltaic device can reduce greatly.But at present common way be with silicon nanowire array after etching on the monocrystal silicon substrate; Directly apply to the preparation of photovoltaic device; The monocrystal silicon substrate of array bottom does not in fact play a role, and only plays the array supporting role, causes the very big waste of silicon base like this.For further reducing the cost of synthetic silicon nanowire array, be badly in need of the development relevant art, make silicon nanowire array can realize large tracts of land etching and transfer.The silicon nanowire array of metal auxiliary etch large tracts of land layering remaining monocrystal silicon substrate after shifting can be utilized after polishing once more, thereby realizes making full use of of silicon base.And be transferred to flexible substrates through silicon nanowires being received array, also help to realize the application of flexible photovoltaic device.People such as Jeffrey M. Weisse adopted the method for 75 ℃ of hot-water soaks processing to make the catalyst layering in 2010
[1], make the silicon nanowires layering through etching once more.But the Catalyst processing method that adopts is complicated, and the silicon linear diameter is very big, and the silicon line is easy to come off in the solution soaking processing procedure, is unfavorable for the transfer of silicon nanowire array.List of references: [1] J. M. Weisse, D. R. Kim, C. H. Lee, and X. L. Zheng, Nano Lett., 11,1300-1305 (2011).
Summary of the invention
For the bulk silicon that makes the metal auxiliary etch prepare silicon nanowire array is fully used; And silicon nanowire array is used to make the flexible silicon nano-device; The invention provides a kind of metal auxiliary silicon nano-wire array large tracts of land layering etching and transfer method, utilize metal catalytic electroless plating chemical method, prepare on the basis of silicon nanowire array an etching; With silicon nanowire array annealing in process in air; Make metal catalyst particles fusing and part be attached on the array sidewall, lateral etching takes place in secondarily etched, thereby in silicon nanowire array, produce a lateral fault.Then utilize certain means that it is peeled off, the silicon nanowire array after peeling off is as preparation flexible silicon nano-device.
The apprizing system of the apprizing system appearance treatment plant of appearance treatment plant reaches above-mentioned technique effect for realizing above-mentioned technical purpose, and the present invention realizes through following technical scheme:
A kind of metal auxiliary silicon nano-wire array large tracts of land layering etching and transfer method: the lower characteristics of fusing point of utilizing the Ag nano particle; Wet etching is prepared nanoscale Ag catalyst heat treated in air that silicon nanowire array uses; Ag nanocatalyst particles fuse is separated; Make part A g nano particle be attached on the sidewall of silicon nanowire array, in etching reaction once more, lateral etching can take place in the Ag nano particle that sticks; Thereby make silicon nanowire array through horizontal neat tomography of secondarily etched generation, its specific operation process is:
Step 1) is got the polishing monocrystalline silicon piece of any crystal orientation and doping content, after being cut into area and being about 1cm * 1cm fritter, is V (H through acetone ultrasonic cleaning l0min, alcohol ultrasonic cleaning l0min, volume ratio successively at room temperature
2O
2): V (H
2SO
4The ultrasonic l0min of)=1:3 cleaning fluid cleans silicon chip, and it is subsequent use to utilize nitrogen to dry up after deionized water is cleaned;
Step 2) silicon chip after will cleaning immerses HF, AgN0
3Concentration is respectively in the mixed solution of 4.6mol/L, 0.02mol/L, makes silicon chip surface plate one deck nanometer Ag particle uniformly, uses the washed with de-ionized water silicon base;
Silicon chip after step 3) plating Ag handles places HF, H
2O
2Solubility is respectively in the etching liquid of 4.6mol/L, 0.4mol/L carries out the etching first time;
After etching afterwash of step 4) silicon base dries up, will have silicon chip 150 ℃ of heated at constant temperature 1h in air of one deck silicon nanowire array;
Put into HF/H after the step 5) heating
2O
2Carry out the etching second time in the etching liquid;
Obtain the silicon nanowire array of layering after the step 6) etching finishes, mode such as use that gummed paper is peeled off is to the silicon nanowire array lift-off processing.
Further, make Ag nanocatalyst particles fuse, about 100 ℃, through experimental verification, the optimized temperature that can make silicon nanowire array produce tomography is about 150 ℃ according to the fusing point of Ag nano particle.
What further, select for use in the specific embodiments is that N (100) resistivity is that 1.5-2 Ω cm and N (100) doping Sb resistivity are the polishing monocrystalline silicon piece of 0.01-0.008 Ω cm.
Further, for the silver-plated time control of silicon chip surface, at HF, AgN0
3Concentration is respectively 4.6mol/L, 0.02mol/L solution reaction time and is controlled in the 20-30s.
Further, to having the silicon chip heat treated of one deck silicon nanowire array after the etching, 150 ℃ of heating 1h in air.
Further, secondarily etched after the heat treated, at HF, H
2O
2Solubility is respectively that etch period is controlled at about 40min in the etching liquid of 4.6mol/L, 0.4mol/L.
Further, the silicon nanowire array that obtains layering is peeled off it, uses normal tape to be bonded at above the silicon chip that obtains the layering silicon nanowire array, uses certain force and obtains silicon nanowire array.
Further, the method not only can etching obtain two-layer silicon nano-array, also can obtain the silicon nanowire array of repeatedly layering, and simultaneously to different crystal orientations, the monocrystalline silicon piece of different levels of doping is suitable for.Empirical tests all is suitable for the monocrystalline silicon piece in (100), (110) and (111) crystal orientation, and is also suitable to the monocrystalline silicon piece of different levels of doping.
The invention has the beneficial effects as follows:
The present invention can provide a kind of method that is used for suitability for industrialized production, can realize making full use of of bulk silicon base material, and the making of flexible silicon nano-device.
Description of drawings
Fig. 1: the reaction mechanism figure of metal auxiliary silicon nano-wire array large tracts of land etching layering.
The specific embodiment
Below with reference to accompanying drawing and combine embodiment, specify the present invention.
Referring to shown in Figure 1:
One, prepare material:
With monoblock N-Si (100) resistivity is that 1.5～2 Ω cm or N-Si (100) resistivity are the polishing monocrystalline silicon piece of 0.01～0.008 Ω cm; Be cut into the fritter that area is about 1cm * 1cm, use acetone ultrasonic cleaning (room temperature l0 min), alcohol ultrasonic cleaning (room temperature l0 min), cleaning fluid V (H then successively
2O
2): V (H
2SO
4)=1:3 ultrasonic cleaning (room temperature l0 min) cleans up silicon chip subsequent use with deionized water at last.Preparation HF, AgN0
3Concentration is respectively 4.6mol/L, 0.02mol/L solution and HF, H
2O
2Solubility is respectively the etching liquid of 4.6mol/L, 0.4mol/L.
Two, chemical method plating Ag nanoparticle catalyst:
Silicon chip is put into HF, AgN0
3Concentration is respectively in 4.6mol/L, the 0.02mol/L solution, and burnishing surface reacts 20～30s and makes silicon chip surface cover one deck nanoscale Ag particle uniformly as catalyst up, uses the washed with de-ionized water substrate.
Three, preparation silicon nanowire array:
Silicon chip behind the plating Ag nanocatalyst is put into HF, H
2O
2Concentration is respectively in the etching liquid of 4.6mol/L, 0.4mol/L, reacts 30 min, obtains the silicon nanowire array that length is about 15 μ m, with washed with de-ionized water and use N
2Dry up.
Four, the silicon nanowire array that adds the hot preparation layering in the air:
Have silicon chip 150 ℃ of heated at constant temperature 1 h in air of one deck silicon nanowire array after the etching, put into HF, H after the heating
2O
2Concentration is respectively the secondarily etched 35min of etching liquid of 4.6mol/L, 0.4mol/L, takes out the back and cleans up back N with deionized water
2Dry up.The heating for multiple times etching can obtain repeatedly layering.The Ag catalyst is used HNO
3To remove, washed with de-ionized water N2 dries up.Sample preparation can be observed the layering result with ESEM.
Five, peeling off of silicon nanowire array:
The silicon chip that has silicon nanowire array after layering is handled is attached to burnishing surface etching gained silicon nanowire array top with adhesive tape, and the application of force is peeled off and obtained silicon nanowire array.
Claims (7)
1. metal auxiliary silicon nano-wire array large tracts of land layering etching and transfer method is characterized in that, the silicon nanowire array of wet etching preparation uses the nanometer-level silver particle to make catalyst; Utilize the lower characteristics of fusing point of Ag nano particle; Heating makes Ag nanocatalyst particle fusing take place and shrink in air, thereby makes the Ag nano particle partly be attached on the silicon nanowire array sidewall, the Ag nano particle trend lateral etching that sticks in the etching once more; Thereby make silicon nanowire array produce tomography; The method can realize that repeatedly the layering agent is peeled off, and also is applicable to the monocrystalline silicon piece of different crystal orientations and different levels of doping simultaneously, and its specific operation process is:
Step 1) the method is applicable to the monocrystalline silicon piece of different crystal orientations and different levels of doping; During concrete operations, choosing the monocrystalline silicon piece of any one crystal orientation and doping content, after being cut into area and being about 1cm * 1cm fritter, is V (H through acetone ultrasonic cleaning l0min, alcohol ultrasonic cleaning l0min, volume ratio at room temperature successively
2O
2): V (H
2SO
4)=1:3 cleaning fluid ultrasonic cleaning l0min cleans up the back with silicon chip and dries up subsequent use with nitrogen;
Step 2) silicon chip that cleans up is immersed HF, AgN0
3Concentration is respectively in the mixed solution of 4.6mol/L, 0.02mol/L and makes silicon chip surface plate one deck nanometer Ag stratum granulosum uniformly, with deionized water substrate is cleaned up again;
Silicon chip after step 3) will be handled places HF, H
2O
2Solubility is respectively etching a period of time in the etching liquid of 4.6mol/L, 0.4mol/L, forms the ground floor silicon nanowire array;
The silicon chip that will have one deck silicon nanowire array after etching of step 4) is cleaned with deionized water and is dried up, and in air 150 ℃ of heated at constant temperature 1h;
Silicon chip after the step 5) heating is put into HF/H
2O
2Carry out secondarily etchedly in the etching liquid, etch period is by the decision of the height of the second layer array of hope, but the oversize reaction time can cause the ground floor silicon nanowire array to come off, the reaction time of therefore optimizing is about 40 min;
Obtain the silicon nanowire array of layering after the step 6) etching finishes, mode such as use that gummed paper is peeled off is to silicon nanowire array lift-off processing successively.
2. metal auxiliary silicon nano-wire array large tracts of land layering etching according to claim 1 and transfer method; It is characterized in that: utilize the lower characteristics of Ag nano particle fusing point; In air, heat; Make catalyst A g nano particle melt portions be attached on the sidewall of silicon nanowire array, the temperature that can make the silicon nanowire array reaction generate tomography is about 150 ℃.
3. metal auxiliary silicon nano-wire array large tracts of land layering etching according to claim 1 and transfer method; It is characterized in that: the method is applicable to the monocrystalline silicon piece of different crystal orientations and different levels of doping, and to be N (100) resistivity be 1.5-2 Ω cm and N (100) the doping Sb resistivity polishing monocrystalline silicon piece as 0.01-0.008 Ω cm to the silicon chip that uses in the specific embodiments.
4. metal auxiliary silicon nano-wire array large tracts of land layering etching according to claim 1 and transfer method is characterized in that: for the silicon chip surface plating control of nanocatalyst silver time, silicon chip is at HF, AgN0
3Concentration is respectively that the reaction time is controlled in the 20-30s in 4.6mol/L, the 0.02mol/L solution.
5. metal auxiliary silicon nano-wire array large tracts of land layering etching according to claim 1 and transfer method is characterized in that: to silicon chip heat treated in air after etching, at 150 ℃ of following heated at constant temperature 1h.
6. according to the said metal auxiliary silicon of claim 1 nano-wire array large tracts of land layering etching and transfer method, it is characterized in that: in air after the heat treated secondarily etched after, at HF, H
2O
2Solubility is respectively that etch period is controlled at about 40min in the etching liquid of 4.6mol/L, 0.4mol/L.
7. according to the said metal auxiliary silicon of claim 1 nano-wire array large tracts of land layering etching and transfer method; It is characterized in that: obtain behind the silicon nanowire array of layering it being peeled off; Use common gummed paper to be bonded at layering silicon nanowire array top; Use certain force and gummed paper is torn obtain silicon nanowire array, the method not only can etching obtain two-layer silicon nanowire array, also can etching obtains multilayer and successively peels off.
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